WO2018224092A1 - Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method - Google Patents
Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method Download PDFInfo
- Publication number
- WO2018224092A1 WO2018224092A1 PCT/DE2018/100533 DE2018100533W WO2018224092A1 WO 2018224092 A1 WO2018224092 A1 WO 2018224092A1 DE 2018100533 W DE2018100533 W DE 2018100533W WO 2018224092 A1 WO2018224092 A1 WO 2018224092A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- tablets
- pellets
- nanoparticulate
- press
- pressing
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
Definitions
- the invention relates to a compressed tablet / pellet production process of nanoparticulate pressed tablets / pellets of synthetic and / or natural materials, comprising the steps:
- the invention relates to a pressed tablet or a pellet and uses thereof.
- micro-analytical methods for elemental concentration determinations directly on solids are becoming more and more universally applicable and are widely used, e.g. in research, materials quality assurance or mining exploration.
- homogeneous natural materials e.g. Crystals
- Homogeneous synthetic glasses are difficult and can not be produced by all substances.
- Standard reference materials are required which should be as similar in their properties as possible to those of the unknown samples (matrix matching). These SRM must be so homogeneous at each point that microanalyses with eg 1 ⁇ to 100 ⁇ spatial resolution always the same result within a given
- SRM so far find natural or synthetic glasses, natural or synthetic minerals, metals or metal alloys, powder pressed tablets of natural or synthetic substances or mixtures of substances.
- Persistent pressed tablets made of powders have so far been produced only with the addition of binders.
- Composition (50+ elements) is hardly possible.
- the object of the invention is to demonstrate new possibilities for producing homogeneous standards for a variety of materials.
- Press tablets / pellets made of synthetic or natural materials are to be produced according to a newly developed grinding and pressing process. These tasks are solved with the corresponding feature combinations according to the main claim and according to the independent claims.
- the compressed tablet / pellet manufacturing process of nanoparticulate pressed tablets / pellets of synthetic and / or natural materials comprises the steps:
- the at least one aliquot is selected for pressing from the dried and rehomogenized nanopowder
- a nanoparticulate powder with grain sizes D90 ⁇ 1 ⁇ is formed.
- Nanoparticles are produced using this top-down principle, which can be pressed to form stable tablets without further binders.
- the very small particle sizes ensure excellent homogeneity down to the micrometer range.
- the nano-tablets also offer better properties for measurements with X-ray fluorescence (X-ray scanner) than previously used powder compacts. This will prove the
- Isotope composition The this-world manufacturing process includes an ultra-fine grinding, also referred to as "top-down” principle, nanoparticles, followed by freeze-drying, and the pressing of the nanopowder, in particular with sapphire disks in a preferably programmable high-pressure press.
- This method allows the production of stable pressed tablets of synthetic and / or natural materials, which are converted into nanoparticles, according to the top-down principle, which also makes very complex compositions
- the nanoparticulate powder having particle sizes of 30-150 nm with D90 ⁇ 1 ⁇ m is formed.
- the extremely small particle size in this case allows a very good homogenization of substances / mixtures of substances (10-100 ⁇ scale).
- the pressing of the aliquot is preferably carried out in a high-pressure press in the working range of 2 to 80 1, 3 to 40 or especially 5 to 20 1.
- a sapphire disk can be placed between the powder and the die.
- the wet milling may be carried out with a liquid, wherein the liquid may be water, deionized water and / or an organic solvent.
- the main parameters that change depending on the material, the amount of water and the grinding time, with other parameters such as
- Revolution speed (acceleration), etc. can be additionally varied.
- the following milling protocols for geological / environmental materials are listed:
- Carbonate / phosphate 15 min, 10 ml D.I. water
- Press tablets / pellet manufacturing processes of nanoparticulate pressed tablets / pellets of synthetic and / or natural materials are also worthy of protection.
- the foregoing pressed tablets / pellets prepared by one of the foregoing press-tablet / pellet manufacturing methods of nanoparticulate pressed tablets / pellets of synthetic and / or natural materials may be used as direct medium
- Solid analysis can be used.
- the surface is extremely flat and smooth (roughness ⁇ 30-150 nm); Compacts are ultra-homogeneous, stable and have an extremely smooth and even surface;
- micro-SRM micro-SRM
- Fig. 1 is a schematic representation of an embodiment of the known in the prior art manufacturing method
- Fig. 2 is a schematic representation of an embodiment of the disclosed here
- Fig. 1 is a schematic representation of an embodiment of the known in the prior art manufacturing process is shown.
- the starting material p is finely ground ( ⁇ 75 ⁇ m) and in the
- cellulose, wax, boric acid, organic compounds, etc. mixed A (b) and homogenized H. Subsequently, an aliquot thereof (p + b) H is added in a high pressure hydraulic press of 5 to 20 liters of a tablet / pellet t (p + b) H pressed P.
- Fig. 2 shows a schematic representation of an embodiment of the manufacturing method disclosed herein.
- 3-4 g of finely ground powder p of the original material are weighed in a grinding cup, for example made of agate, under a so-called clean bench in a particle-free atmosphere.
- the grinding bowl already contains a certain amount of grinding balls made of agate, with diameter and total mass of the grinding balls according to the material (grinding protocol).
- DIW de-ionized water
- the amount depends on the material to be ground (grinding protocol) and is such that during the suspension, a suspension with oil-like viscosity is formed. Subsequently, a closure of the grinding bowl and insertion into a ball mill.
- the grinding time is material-specific and has been optimized for a number of materials (milling protocol). This produces particles with particle sizes in the nanometer range (30-150 nm, ⁇ 90 ⁇ 1 ⁇ ).
- the ready-milled nanopowder p M is rinsed as a suspension with DIW from the balls and the grinding bowl and transferred with a pipette into a pre-cleaned plastic cup.
- the plastic cup with the suspension (about 50-100 ml) is flash frozen at -80 ° C and then dried in a freeze dryer G over 72-96 h.
- the dried nanopowder PMG is transferred to a hand mortar made of agate and rehomogenizes H.
- the rehomogenized nanopowder P M GH is weighed into the die (approximately 600 mg for a 13 mm diameter tablet), which is then inserted into a programmable hydraulic tablet press, and the powder is then added at 10 t / cm 2 (for 13 mm diameter Press protocol) over 1 minute compressed P.
- a sapphire disc is placed between powder p M G and ram.
- Tablets t (p MG H) of various diameters (eg 5, 10, 13, 32 mm) were prepared. LIST OF REFERENCE NUMBERS
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Medicinal Preparation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA3066477A CA3066477C (en) | 2017-06-08 | 2018-06-05 | Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method |
AU2018279770A AU2018279770B2 (en) | 2017-06-08 | 2018-06-05 | Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method |
US16/619,501 US11656158B2 (en) | 2017-06-08 | 2018-06-05 | Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method |
EP18736786.7A EP3635362A1 (en) | 2017-06-08 | 2018-06-05 | Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102017112691.0A DE102017112691B4 (en) | 2017-06-08 | 2017-06-08 | Production of nanoparticulate pressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and pressing process |
DE102017112691.0 | 2017-06-08 |
Publications (1)
Publication Number | Publication Date |
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WO2018224092A1 true WO2018224092A1 (en) | 2018-12-13 |
Family
ID=62814761
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/DE2018/100533 WO2018224092A1 (en) | 2017-06-08 | 2018-06-05 | Production of nanoparticulate compressed tablets (pellets) from synthetic or natural materials using a specially developed grinding and compressing method |
Country Status (6)
Country | Link |
---|---|
US (1) | US11656158B2 (en) |
EP (1) | EP3635362A1 (en) |
AU (1) | AU2018279770B2 (en) |
CA (1) | CA3066477C (en) |
DE (1) | DE102017112691B4 (en) |
WO (1) | WO2018224092A1 (en) |
Families Citing this family (2)
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WO2024186797A1 (en) * | 2023-03-07 | 2024-09-12 | Gtf, Llc | Method of processing hops plants into pellets, feedstock, and fertilizer |
US11782040B1 (en) * | 2023-05-12 | 2023-10-10 | Michele Glinn | Cannabis potency testing method |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004077521A2 (en) * | 2003-02-26 | 2004-09-10 | The Regents Of The University Of California | Ceramic materials reinforced with single-wall carbon nanotubes as electrical conductors |
EP1621526A1 (en) * | 2004-07-02 | 2006-02-01 | Consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali (INSTM) | A method of preparing nanostructured composite ceramic materials |
WO2006024098A1 (en) * | 2004-09-01 | 2006-03-09 | Advanced Nanotechnology Limited | A zirconia ceramic |
US20080135798A1 (en) * | 2006-12-07 | 2008-06-12 | Jae Ho Jeon | Nano-Size Lead-Free Piezoceramic Powder and Method of Synthesizing the Same |
-
2017
- 2017-06-08 DE DE102017112691.0A patent/DE102017112691B4/en active Active
-
2018
- 2018-06-05 CA CA3066477A patent/CA3066477C/en active Active
- 2018-06-05 AU AU2018279770A patent/AU2018279770B2/en active Active
- 2018-06-05 US US16/619,501 patent/US11656158B2/en active Active
- 2018-06-05 WO PCT/DE2018/100533 patent/WO2018224092A1/en unknown
- 2018-06-05 EP EP18736786.7A patent/EP3635362A1/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004077521A2 (en) * | 2003-02-26 | 2004-09-10 | The Regents Of The University Of California | Ceramic materials reinforced with single-wall carbon nanotubes as electrical conductors |
EP1621526A1 (en) * | 2004-07-02 | 2006-02-01 | Consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali (INSTM) | A method of preparing nanostructured composite ceramic materials |
WO2006024098A1 (en) * | 2004-09-01 | 2006-03-09 | Advanced Nanotechnology Limited | A zirconia ceramic |
US20080135798A1 (en) * | 2006-12-07 | 2008-06-12 | Jae Ho Jeon | Nano-Size Lead-Free Piezoceramic Powder and Method of Synthesizing the Same |
Non-Patent Citations (3)
Title |
---|
AURÉLIE CARDIN: "High throughput method for the development of bulk lead free piezoelectric ceramics", 24 June 2009 (2009-06-24), XP055509903, Retrieved from the Internet <URL:https://scidok.sulb.uni-saarland.de/bitstream/20.500.11880/22639/1/dissACardin_210609.pdf> [retrieved on 20180925], DOI: 10.22028/D291-22583 * |
D. GARBE-SCHÖNBERG; S. MÜLLER: "J. Anal. At. Spectrom.", vol. 29, 16 April 2014, THE ROYAL SOCIETY OF CHEMISTRY, article "Nano-particulate pressed powder tablets for LA-ICP-MS", pages: 990 |
DIETER GARBE-SCHÖNBERG ET AL: "Nano-particulate pressed powder tablets for LA-ICP-MS", JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, vol. 29, no. 6, 1 January 2014 (2014-01-01), pages 990 - 1000, XP055509904, ISSN: 0267-9477, DOI: 10.1039/C4JA00007B * |
Also Published As
Publication number | Publication date |
---|---|
CA3066477C (en) | 2021-12-14 |
AU2018279770A1 (en) | 2019-12-19 |
DE102017112691B4 (en) | 2020-02-27 |
CA3066477A1 (en) | 2018-12-13 |
US20200140341A1 (en) | 2020-05-07 |
AU2018279770B2 (en) | 2021-01-28 |
DE102017112691A1 (en) | 2018-12-13 |
EP3635362A1 (en) | 2020-04-15 |
US11656158B2 (en) | 2023-05-23 |
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